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Method for enriching leucomalachite green and leucogentian violet in aquatic products

A technology of leuco malachite green and leuco crystal violet is applied in measuring devices, instruments, scientific instruments and other directions, which can solve problems such as workload consumption, save materials, reduce organic solvents, and reduce detection errors.

Inactive Publication Date: 2013-10-16
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] At present, in the food safety detection and analysis of trace analytes, nearly half of the errors come from the pretreatment of samples, while the errors that really come from instrument detection are less than one-third, and nearly 70% of the workload is spent In the pre-processing stage of the sample
However, this method is still not suitable for the enrichment analysis of fat-soluble LMG in aquatic products.

Method used

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  • Method for enriching leucomalachite green and leucogentian violet in aquatic products
  • Method for enriching leucomalachite green and leucogentian violet in aquatic products
  • Method for enriching leucomalachite green and leucogentian violet in aquatic products

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Embodiment 1

[0043] The C of embodiment 1 particle diameter 100nm 18 Preparation of polystyrene microspheres

[0044] Using surface amino-modified polystyrene magnetic balls as raw materials:

[0045] 1) Amination of carboxylated magnetic spheres: disperse commercialized polystyrene magnetic spheres with a diameter of 100nm and surface carboxyl modification (product of Shanghai Aorun Micro-Nano New Material Technology Co., Ltd., product number PM3-008) in boron In salt buffer solution (pH4.0), according to the molar ratio of carboxyl group: 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide: N-hydroxysulfosuccinimide on the magnetic ball =1:3:6 Add 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide and N-hydroxysulfosuccinimide respectively, and shake for 2 hours to activate the carboxyl group on the magnetic ball. Take ethylenediamine, add a dose of 300 to 800 times the molar number of carboxyl groups, adjust the pH to 8 with concentrated hydrochloric acid, add activated magnetic balls, shake and...

Embodiment 2

[0048] The C of embodiment 2 particle size 180nm 18 Preparation of polystyrene magnetic spheres

[0049] In step (1), commercialized polystyrene magnetic balls with a diameter of 180nm and surface carboxyl modification (product of Shanghai Aorun Micro-Nano New Material Technology Co., Ltd., product number PM3-020) are used as raw materials;

[0050] In step (2), take 700 μL of oleic acid and add it to 3.5 mL of anhydrous tetrahydrofuran, according to the molar ratio of oleic acid:N,N-dicyclohexylcarbodiimide:N-hydroxysuccinimide=1:3:6 respectively Add N,N-dicyclohexylcarbodiimide and N-hydroxysuccinimide, shake vigorously for 2 hours, centrifuge to get the supernatant, add triethylamine to adjust the pH value of the solution to 9;

[0051] In step (3), 500 mg of polystyrene magnetic spheres with a particle size of 180 nm and modified by surface amino groups in step (1) were washed twice with anhydrous tetrahydrofuran in advance, and then added to oleic acid with activated car...

Embodiment 3

[0053] The C of embodiment 3 particle diameter 70nm 18 Preparation of silica magnetic spheres

[0054] Using a magnetic ball with a silica shell as a carrier:

[0055] 1) Synthesis of silica magnetic spheres with a particle size of 70nm. Referring to the literature (Yan F, Li J, Zhang J, Liu F, Yang W.J.Nanopart.Res., 2009, 11(2):289~296), the chemical co-precipitation method was used to synthesize superparamagnetic Fe 3 o 4 single nanoparticle. Fe 3 o 4 The surface of nanoparticles was acidified with oil, washed with absolute ethanol and dried with nitrogen gas. Suspend 3g Fe in 2.0mL cyclohexane 3 o 4 Nanoparticles to obtain ferrofluid, transfer the ferrofluid into 400mL, 0.01M NaHCO containing 0.5% SDS 3 In the solution, 300W (25KHz) power continued ultrasonic emulsification for 30min to form a fine emulsion; reflux at 70°C for 12h to remove cyclohexane to obtain Fe 3 o 4 Nanoparticle clusters; Magnetic separation of Fe 3 o 4 Nanoparticle clusters, suspended Fe...

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Abstract

The invention discloses a method for enriching leucomalachite green and leucogentian violet in aquatic products, and relates to a new method for preprocessing a sample in the field of the safe analysis of foods. The method comprises the following steps: preprocessing a sample, adding super-paramagnetic nanometer or submicron magnetic spheres with the surfaces modified with a C18 alkyl chain for adsorption, eluting, and collecting the obtained eluate; and directly adding the eluate to a liquid chromatograph or a liquid chromatograph-mass spectrometer, and quantitatively analyzing the contents of leucomalachite green and leucogentian violet. The method has the characteristics of simple operation flow, high extraction and recovery rates, less consumption of elution solvents, and no need of rotary evaporation.

Description

technical field [0001] The invention relates to sample pretreatment in the field of food safety analysis, in particular to a C 18 A method for enriching leuco malachite green and leuco crystal violet in aquatic products by magnetic balls. Background technique [0002] Malachite green (MG) is a basic triphenylmethane dye. Because of its strong antibacterial and antiparasitic effects and low price, it is widely used in the disinfection of pond water and the prevention and treatment of saprolegniasis, gill rot and parasitic diseases in fish. MG is easily absorbed by aquatic products and rapidly metabolized into fat-soluble leuco malachite green (LMG) in the body. LMG has potential carcinogenic, teratogenic, mutagenic and other hazards. Because LMG has a long half-life in aquatic products, it can enter the human body through the food chain. [0003] Crystal violet is a dye-type fungicide similar in structure and properties to malachite green. It will also be rapidly metaboli...

Claims

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Application Information

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IPC IPC(8): G01N30/08
Inventor 郭亮熊勇华许恒毅陈雪岚魏华徐峰赖卫华
Owner NANCHANG UNIV
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